宣肺祛风合剂的质量标准研究

Study on the quality standards of Xuanfei Qufeng Heji

目的制定宣肺祛风合剂的质量标准。方法采用薄层色谱法(TLC)对处方中的前胡、钩藤进行鉴别;采用高效液相色谱法(HPLC)测定方中麻黄碱类成分含量,Supelco ODS C18柱(250 mm×4.6 mm,5μm),流动相:乙腈-0.2%磷酸水溶液(3∶97);检测波长:210 nm。柱温:30℃;流速:1.0 mg·L^(-1)。结果前胡、钩藤TLC鉴别斑点清晰,阴性无干扰,可作为定性鉴别;HPLC测定盐酸麻黄碱在0.843 75~54.00 mg·L^(-1)范围内,与峰面积性关系良好,回归方程为Y=19.48X+12.554,r2=0.999 9,平均回收率为98.2%,RSD=2.4%(n=5);盐酸伪麻黄碱在0.781 25~50.00 mg·L^(-1)范围内,与峰面积的积分值呈良好的线性关系,回归方程Y=19.816X+12.468(r2=0.999 9),平回收率均为97.9%,RSD=1.7%(n=5)。结论TLC鉴别方法操作简单,专属性强;HPLC含量测定方法准确、重现性良好,可作为该制剂的质量控制方法。

Objective To establish the quality standard of xuanfei qufeng heji. Methods Peucedanum praeruptorum Dunn and Ramulus Uncariae Cum Uncis were identified by TLC. The contents of ephedrine hydrochloride and pseudoephedrine hydrochloride were examined by HPLC. The optimal conditions of the separation and detection were achieved on a supelco ODS C18column(4. 6 mm × 250 mm,5 μm) with a mobile phase consisting of metha acetonitrile-0. 2% phosphoric acid solution(3∶ 97) at the detective wavelength of210 nm. The column temperature was 30 ℃ and the flow rate was 1 m L·min-1. Results TLC spots of Peucedanum praeruptorum Dunn. and Ramulus Uncariae Cum Uncis were clear and negative without interference,which can be used as qualitative method. The contents of ephedrine hydrochloride had a good linear relation with(r2= 0. 999 9),when ranging from 0. 843 7-54. 00 mg·L^(-1)and equation was Y = 19. 816 X + 2. 554,The average recovery of ephedrine hydrochloride was 98. 2% and RSD was 2. 4%(n = 5). The contents of pseudoephedrine hydrochloride had a good linear relation with(r2= 0. 999 9) when ranging from 0. 781 25-50. 00 mg·L^(-1)and equation was Y = 19. 816 X + 12. 468,The average recovery of pseudoephedrine hydrochloride was 97. 9% and RSD was 1. 7%(n = 5) Conclusions The TLC method is simple and has good specificity. The HPLC method is acute and repeatable. So the two methods can be used as the quality control for this preparation.